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Double-column solid phase extraction method of nitrogen-containing compounds in diesel oil

A solid-phase extraction method, nitrogen compound technology, applied in chemical instruments and methods, refined hydrocarbon oil, petroleum industry, etc., can solve the problems of large separation crossover, large solvent consumption, long processing time, etc., and achieve small separation crossover. , The amount of stationary phase and solvent is less, and the effect of improving work efficiency

Active Publication Date: 2017-01-11
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention can solve the problems of large amount of separation and crossover between components, large amount of solvent and long processing time when traditional column chromatography is used for separation and enrichment of nitrogen-containing compounds in diesel oil

Method used

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  • Double-column solid phase extraction method of nitrogen-containing compounds in diesel oil
  • Double-column solid phase extraction method of nitrogen-containing compounds in diesel oil
  • Double-column solid phase extraction method of nitrogen-containing compounds in diesel oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 3.5 g of silica gel-acidic alumina stationary phase with an acidic alumina content of 10 wt % was loaded in the solid phase extraction column A, and wetted with 2 mL of the first eluent (n-pentane). 2.5 g of silica gel-basic alumina stationary phase with a basic alumina content of 60 wt % was loaded in the solid phase extraction column B. The activation temperature of silica gel is 80°C and the activation time is 6 hours, the activation temperature of acidic alumina is 350°C and the activation time is 7 hours, the activation temperature of basic alumina is 350°C and the activation time is 6 hours.

[0057] Use a pipette gun to take 2mL of Qingyang Petrochemical catalytic cracked diesel oil into the upper part of solid phase extraction column A and be completely absorbed by the stationary phase. The SPE cartridge was flushed with 6 mL of the first eluent (n-pentane) to obtain saturated hydrocarbons (component 1). Rinse the solid-phase extraction column with 10 mL of the...

Embodiment 2

[0071] 3.5 g of silica gel-acidic alumina stationary phase with an acidic alumina content of 30 wt % was filled in the solid phase extraction column A, and wetted with 2 mL of the first eluent (n-hexane). 2.5 g of silica gel-basic alumina stationary phase with a basic alumina content of 40 wt % was loaded in the solid phase extraction column B. The activation temperature of silica gel is 100°C and the activation time is 4 hours, the activation temperature of acidic alumina is 400°C and the activation time is 5 hours, the activation temperature of basic alumina is 400°C and the activation time is 4 hours.

[0072] Use a pipette gun to take 1mL of Karamay petrochemical coked diesel oil and add it to the upper part of solid phase extraction column A and be completely absorbed by the stationary phase. Rinse the SPE column with 8 mL of the first eluent (n-hexane) to obtain saturated hydrocarbons (component 1). Rinse the SPE column with 9 mL of the second eluent (the volume ratio o...

Embodiment 3

[0077] 3.5 g of silica gel-acidic alumina stationary phase with an acidic alumina content of 40 wt % was filled in the solid phase extraction column A, and wetted with 2 mL of the first eluent (n-heptane). 2.5 g of silica gel-basic alumina stationary phase with a basic alumina content of 20 wt % was loaded in the solid phase extraction column B. The activation temperature of silica gel is 120°C and the activation time is 3 hours, the activation temperature of acidic alumina is 450°C and the activation time is 4 hours, the activation temperature of basic alumina is 450°C and the activation time is 2 hours.

[0078] Use a pipette gun to take 5mL of Daqing Petrochemical straight-run diesel oil and add it to the upper part of the solid-phase extraction column A and be completely absorbed by the stationary phase. The SPE cartridge was flushed with 9 mL of the first eluent (n-heptane) to obtain saturated hydrocarbons (component 1). Rinse the SPE column with 7 mL of the second eluen...

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Abstract

A double-column solid phase extraction method of nitrogen-containing compounds in diesel oil comprises the following steps: 1, producing solid phase extraction columns, wherein the stationary phase of the solid phase extraction column A is a silica gel and acidic alumina mixture, and the stationary phase of the solid phase extraction column B is a silica gel and alkaline alumina mixture; and 2, eluting: wetting the solid phase extraction column A by a first eluent, adding a diesel oil sample from an upper layer, flushing the solid phase extraction column A with the first eluent to obtain saturated hydrocarbons, flushing the solid phase extraction column A with a second eluent to obtain aromatic hydrocarbons, flushing the solid phase extraction column A with a third eluent to obtain neutral nitrogen-containing compounds, serially connecting the solid phase extraction column A with the solid phase extraction column B, and flushing the solid phase extraction columns A and B with a fourth eluent to obtain alkaline nitrogen-containing compounds, wherein the column A is arranged above the column B.

Description

technical field [0001] The invention relates to the field of petrochemical industry, in particular to a method for separating and enriching neutral nitrogen-containing compounds and basic nitrogen-containing compounds in a diesel sample by adopting a double-column method of solid-phase extraction. Background technique [0002] Nitrogen-containing compounds in diesel fuel are prone to form nitrogen oxides such as nitrogen dioxide during combustion. Such substances are likely to cause poisoning of motor vehicle exhaust catalysts during the discharge process; after being discharged into the atmosphere, such substances are one of the main pollutants that form acid rain and acid fog; in addition, nitrogen oxides and hydrocarbons can form photochemical smog, and cause damage to the ozone layer. Therefore, reducing the content of nitrogen-containing compounds in diesel oil is a requirement for fuel cleanliness. According to the needs of diesel denitrification process technology d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G25/00B01D15/42B01D15/22G01N30/08G01N30/02
Inventor 史得军薛慧峰肖占敏杨晓彦马晨菲林骏陈泱何京王飞赫丽娜陈芬芬汪艳
Owner PETROCHINA CO LTD
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